CN111072037B - Preparation method of silica aerogel - Google Patents
Preparation method of silica aerogel Download PDFInfo
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- CN111072037B CN111072037B CN202010084311.6A CN202010084311A CN111072037B CN 111072037 B CN111072037 B CN 111072037B CN 202010084311 A CN202010084311 A CN 202010084311A CN 111072037 B CN111072037 B CN 111072037B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
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Abstract
The invention belongs to the technical field of aerogel, in particular to the technical field of silica aerogel, and relates to a preparation method of silica aerogel with better flexibility, which comprises the following steps of preparing methyltrialkoxysilane with a structural formula of R 1 Si(OR 2 ) Mixing the functional silane coupling agent, absolute ethyl alcohol and deionized water, adding an acid solution for hydrolysis, and then adding an alkali compound for condensation to prepare wet gel; after the wet gel is aged, replacing for 2 times by using a cross-linking agent solution, taking out, cross-linking under ultraviolet irradiation, and drying to obtain flexible silica aerogel; wherein R is 1 Independently selected from vinyl or 3-mercaptopropyl, R 2 Independently selected from methyl, ethyl or isopropyl. The silica aerogel disclosed by the invention has good flexibility, can be compressed by 33% or more without breaking, and can keep 93% or more of the original height after being repeatedly compressed for 20 times.
Description
Technical Field
The invention relates to the technical field of aerogel, in particular to the technical field of silica aerogel, and relates to a preparation method of silica aerogel with good flexibility.
Background
Aerogel generally refers to a lightweight nano-solid material in which nano-scale ultrafine particles are mutually aggregated to form a nano-porous network structure, and the network pores are filled with a gaseous dispersion medium. Aerogel is a solid but 99% by volume is a gas.
The silica aerogel is one of the aerogels, has excellent heat insulation performance (the heat conductivity coefficient is as low as below 0.015W/m.k), unique flame-proof burning-through performance, good heat stability (high temperature resistance up to 600 ℃), excellent sound insulation performance, good light transmittance, good chemical stability, environmental protection performance and the like, and is a novel material with very high application potential.
However, silica aerogel has the following disadvantages: (1) The preparation method needs freeze drying or supercritical drying, and has high cost, long period and low efficiency; (2) too low strength and is prone to chipping. Thus, its application is limited.
CN103708476B discloses a method for preparing flexible silica aerogel by using methylalkoxy series silane as a silicon source precursor, which can realize normal pressure drying.
However, there is still a need to develop silica aerogels that are more flexible.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of silica aerogel with good flexibility.
According to the preparation method, the vinyl or sulfhydryl-containing silane coupling agent capable of reacting under ultraviolet irradiation is introduced in the preparation process of the silica aerogel to carry out cohydrolysis, the cross-linking agent is added after ageing to carry out cross-linking, and the silica aerogel with better flexibility is obtained after drying.
The technical scheme adopted by the invention is as follows: methyl trialkoxysilane with a structural general formula of R 1 Si(OR 2 ) Mixing the functional silane coupling agent, absolute ethyl alcohol and deionized water, adding an acid solution for hydrolysis, and then adding an alkali compound for condensation to prepare wet gel; after the wet gel is aged, replacing for 2 times by using a cross-linking agent solution, taking out, cross-linking under ultraviolet irradiation, and drying to obtain flexible silica aerogel; wherein R is 1 Independently selected from vinyl or 3-mercaptopropyl, R 2 Independently selected from methyl, ethyl or isopropyl.
When R is 1 When vinyl, the cross-linking agent uses mercapto silicone oil; when R is 1 In the case of 3-mercaptopropyl, vinyl silicone oil is used as the crosslinking agent.
The beneficial effects of the invention are as follows:
(1) According to the preparation method, the silane coupling agent with the crosslinkable group is introduced into the reaction raw materials to participate in hydrolysis, the crosslinkable group is arranged on the surface of the obtained wet gel, and then the crosslinking agent is introduced through replacement after aging, so that crosslinking is realized under ultraviolet irradiation, a hybrid interpenetrating structure of a silicon dioxide three-dimensional network structure and a polysiloxane three-dimensional network structure is formed, and the flexibility of the silicon dioxide aerogel is improved.
(2) The silica aerogel of the present invention can be compressed 33% or more without breaking, and can maintain 93% or more of the original height after repeated compression for 20 times.
Detailed Description
The technical scheme of the invention is further illustrated and described through the following specific embodiments.
Description of the embodiments
A method for preparing flexible silica aerogel comprises the following steps of preparing methyltrialkoxysilane with a structural formula of R 1 Si(OR 2 ) Mixing the functional silane coupling agent, absolute ethyl alcohol and deionized water, adding an acid solution for hydrolysis, and then adding an alkali compound for condensation to prepare wet gel; after the wet gel is aged, replacing for 2 times by using a cross-linking agent solution, taking out, cross-linking under ultraviolet irradiation, and drying to obtain flexible silica aerogel; wherein R is 1 Independently selected from vinyl or 3-mercaptopropyl, R 2 Independently selected from methyl, ethyl or isopropyl.
Preferably, the alkoxy group is selected from at least one of methoxy, ethoxy and isopropoxy.
Preferably, the molar ratio of the methyltrialkoxysilane to the functional silane coupling agent is 1:0.01-0.2. More preferably, the molar ratio of methyltrialkoxysilane to functional silane coupling agent is 1:0.02-0.1.
Preferably, the volume ratio of the methyltrialkoxysilane, the absolute ethyl alcohol and the deionized water is 1:3-5:0.3-0.6.
The acid solution is added to adjust the pH of the reaction system to 2-3, and the acid solution can be selected from dilute sulfuric acid, nitric acid aqueous solution, hydrochloric acid aqueous solution, oxalic acid aqueous solution or aqueous solution of other acidic substances. The concentration of the acid solution is not limited as long as the amount added is sufficient to bring the pH of the reaction system to 2 to 3 and promote the hydrolysis of the siloxane. In a preferred embodiment, the concentration of the acid solution may be 0.1 to 1mol/L, and the acid solution is selected from a hydrochloric acid solution or an oxalic acid solution.
The alkali compound is at least one selected from ammonia water, sodium carbonate, potassium carbonate, sodium hydroxide, potassium hydroxide and tetrabutylammonium hydroxide in tetramethylammonium hydroxide. The addition of the base compound adjusts the pH of the reaction system to 9-11. The alkali compound may be added either directly or after dilution with water or dissolution.
Aging is to place the wet gel in a water bath environment at 25-60deg.C for 24-72 hr.
Preferably, when R 1 When the cross-linking agent is vinyl, the cross-linking agent solution is an absolute ethyl alcohol solution of a mixture formed by mercaptopropyl silicone oil and a photoinitiator, the concentration of the mercaptopropyl silicone oil is 50-200g/L, and the concentration of the photoinitiator is 1-4g/L.
More preferably, the mercaptopropyl silicone oil has a structural formula of Me 3 SiO(SiMeR 3 O) a (SiMe 2 O) b (SiMeRsO) c SiMe 3 Wherein Me is methyl, R 3 Independently selected from phenyl, methyl, 3-trifluoropropyl, ethyl, n-propyl, isopropyl, isobutyl, n-hexyl, n-octyl, isooctyl, n-dodecyl or n-hexadecyl, rs is 3-mercaptopropyl, a is more than or equal to 0 and less than or equal to 20, b is more than or equal to 10 and less than or equal to 50, and c is more than or equal to 2 and less than or equal to 10.
Preferably, when R 1 In the case of 3-mercaptopropyl, the cross-linking agent solution is an absolute ethyl alcohol solution of a mixture composed of vinyl silicone oil and a photoinitiator, the concentration of the vinyl silicone oil is 50-200g/L, and the concentration of the photoinitiator is 1-4g/L.
More preferably, the vinyl silicone oil has a structural formula of Me 3 SiO(SiMeR 4 O) x (SiMe 2 O) y (SiMeViO) z SiMe 3 Wherein Me is methyl, R 4 Independently selected from phenyl, methyl, 3-trifluoropropyl, ethyl, n-propyl, isopropyl, isobutyl, n-hexyl, n-octyl, isooctyl, n-dodecyl or n-hexadecyl, vi is vinyl, x is more than or equal to 0 and less than or equal to 20, y is more than or equal to 10 and less than or equal to 50, and z is more than or equal to 2 and less than or equal to 10.
More preferably, the photoinitiator is selected from benzoin, benzoin dimethyl ether, benzoin diethyl ether or benzoin butyl ether.
The ultraviolet irradiation crosslinking is carried out under the ultraviolet light with the dominant wavelength of 365nm and the light intensity of 1-10mW/cm for 1-10 minutes.
Preferably, the drying is normal pressure drying, and the drying process is that the drying is performed at 40-60 ℃ for 3-5 hours, 80-100 ℃ for 3-5 hours, and 120-150 ℃ for 2-3 hours.
Example 1
Preparing a cross-linking agent solution 1:100g of structural formula Me 3 SiO(SiMe 2 O) 22.7 (SiMeRsO) 3.5 SiMe 3 The mercaptopropyl silicone oil of (2) and 3g of benzoin dimethyl ether are added into absolute ethyl alcohol to prepare 1L volume, wherein Me is methyl, and Rs is 3-mercaptopropyl.
10ml of methyltrimethoxysilane, 0.21ml of vinyltrimethoxysilane, 35ml of absolute ethyl alcohol and 4ml of deionized water are mixed, hydrochloric acid with the concentration of 0.5mol/L is added to adjust the pH to 2.5 for hydrolysis, and ammonia water is added to adjust the pH to 10 for condensation, so that wet gel is prepared; the wet gel is put in a 35 ℃ water bath for aging for 60 hours, taken out, replaced by the cross-linking agent solution 1 for 2 times, taken out, and cross-linked by irradiation of ultraviolet light with the dominant wavelength of 365nm and the light intensity of 5mW/cm for 3 minutes, dried at 40 ℃ for 5 hours, dried at 90 ℃ for 4 hours and dried at 120 ℃ for 2.5 hours, thus obtaining the silica aerogel 1.
And (3) testing: the height of the silica aerogel 1 is 3.8cm, no crushing exists when the silica aerogel is compressed to the height of 2.5cm for the first time, the height is restored to 3.75cm after the pressure is released, the pressure is released after the silica aerogel is continuously compressed to the height of 2.5cm, and the height of the aerogel is 3.6cm after the silica aerogel is repeatedly compressed for 20 times.
Therefore, the elastic change rate of the silica aerogel 1 was (3.8-2.5)/3.8X100% = 34.2%,
the height retention was 3.6/3.8x100% = 94.7%.
Example 2
10ml of methyltrimethoxysilane, 0.5ml of vinyltrimethoxysilane, 40ml of absolute ethyl alcohol and 4.5ml of deionized water are mixed, hydrochloric acid with the concentration of 0.5mol/L is added to adjust the pH value to 2.5 for hydrolysis, ammonia water is added to adjust the pH value to 10 for condensation, and wet gel is prepared; the wet gel was aged in a water bath at 35℃for 60 hours, then taken out, replaced with the crosslinking agent solution 1 of example 1 for 2 times, and then taken out, crosslinked by irradiation with ultraviolet light having a dominant wavelength of 365nm and a light intensity of 5mW/cm for 3 minutes, dried at 40℃for 5 hours, dried at 90℃for 4 hours, and dried at 120℃for 2.5 hours, to obtain silica aerogel 2.
And (3) testing: the height of the silica aerogel 2 is 3.4cm, no crushing exists when the silica aerogel is compressed to the height of 2.1cm for the first time, the height is restored to 3.35cm after the pressure is released, the pressure is released after the silica aerogel is continuously compressed to the height of 2.1cm, and the height of the aerogel is 3.25cm after the silica aerogel is repeatedly compressed for 20 times.
Therefore, the elastic change rate of the silica aerogel 2 was (3.4-2.1)/3.4X100% = 38.2%,
the height retention rate was 3.2/3.4×100% =94.1%.
Example 3
10ml of methyltriethoxysilane, 0.8ml of vinyltriethoxysilane, 37ml of absolute ethanol and 4ml of deionized water are mixed, hydrochloric acid with the concentration of 1mol/L is added to adjust the pH to 2.5 for hydrolysis, and ammonia water is added to adjust the pH to 10.5 for condensation, so that wet gel is prepared; the wet gel was aged in a water bath at 50℃for 30 hours, then taken out, replaced with the crosslinking agent solution 1 of example 1 for 2 times, and then taken out, crosslinked by irradiation with ultraviolet light having a dominant wavelength of 365nm and a light intensity of 5mW/cm for 4 minutes, dried at 40℃for 4 hours, dried at 90℃for 5 hours, and dried at 120℃for 2 hours, to obtain silica aerogel 3.
And (3) testing: the height of the silica aerogel 3 is 4.5cm, no crushing exists when the silica aerogel is compressed to the height of 2.9cm for the first time, the height is restored to 4.4cm after the pressure is released, the pressure is released after the silica aerogel is continuously compressed to the height of 2.9cm, and the height of the aerogel is 4.2cm after the silica aerogel is repeatedly compressed for 20 times.
Therefore, the elastic change rate of the silica aerogel 3 was (4.5-2.9)/4.5X100% = 35.5%,
the height retention was 4.2/4.5×100% =93.3%.
Example 4
Preparing a cross-linking agent solution 2:120g of structural formula Me 3 SiO(SiMePhO) 7.2 (SiMe 2 O) 15.6 (SiMeViO) 4.1 SiMe 3 The vinyl silicone oil of (2) and 3g of benzoin dimethyl ether were added to absolute ethanol to prepare 1L volume, wherein Me is methyl, ph is phenyl, and Vi is vinyl.
10ml of methyltrimethoxysilane, 1.3ml of 3-mercaptopropyl trimethoxysilane, 50ml of absolute ethyl alcohol and 5ml of deionized water are mixed, oxalic acid with the concentration of 0.5mol/L is added to adjust the pH value to 2.5 for hydrolysis, and ammonia water is added to adjust the pH value to 10 for condensation, so that wet gel is prepared; the wet gel is put into a water bath at 35 ℃ for aging for 55 hours, then is taken out, is replaced by a cross-linking agent solution 2 for 2 times, is taken out, is cross-linked by irradiation of ultraviolet light with the dominant wavelength of 365nm and the light intensity of 3mW/cm for 6 minutes, is dried at 40 ℃ for 4 hours, is dried at 90 ℃ for 4 hours, and is dried at 120 ℃ for 3 hours, thus obtaining the silica aerogel 4.
And (3) testing: the height of the silica aerogel 4 is 3.9cm, no crushing exists when the silica aerogel is compressed to the height of 2.6cm for the first time, the height is restored to 3.8cm after the pressure is released, the pressure is released after the silica aerogel is continuously compressed to the height of 2.6cm, and the height of the aerogel is 3.7cm after the silica aerogel is repeatedly compressed for 20 times.
Therefore, the elastic change rate of the silica aerogel 4 was (3.9-2.6)/3.9X100% = 33.3%,
the height retention was 3.7/3.9×100% =94.9%.
Example 5
10ml of methyltriethoxysilane, 1.8ml of 3-mercaptopropyl triethoxysilane, 45ml of absolute ethanol and 5ml of deionized water are mixed, oxalic acid with the concentration of 1mol/L is added to adjust the pH value to 3 for hydrolysis, sodium hydroxide is added to adjust the pH value to 10 for condensation, and wet gel is prepared; the wet gel was aged in a water bath at 40℃for 5 hours, then taken out, replaced with the crosslinking agent solution 2 of example 4 for 2 times, and then taken out, crosslinked by irradiation with ultraviolet light having a dominant wavelength of 365nm and a light intensity of 3mW/cm for 6 minutes, dried at 40℃for 3 hours, dried at 90℃for 3.5 hours, and dried at 120℃for 3 hours, to obtain silica aerogel 5.
And (3) testing: the height of the silica aerogel 5 is 3.5cm, no crushing exists when the silica aerogel is compressed to the height of 2.2cm for the first time, the height is restored to 3.4cm after the pressure is released, the pressure is released after the silica aerogel is continuously compressed to the height of 2.2cm, and the height of the aerogel is 3.3cm after the silica aerogel is repeatedly compressed for 20 times.
Therefore, the elastic change rate of silica aerogel 5 was (3.5-2.2)/3.5X100% = 37.1%,
the height retention was 3.5/3.7x100% = 94.6%.
The foregoing has shown and described the basic principles, features and advantages of the invention. It will be appreciated by persons skilled in the art that the present invention is not limited to the embodiments described above, which are preferred embodiments of the present invention, and the scope of the invention is not limited thereto, i.e. equivalent changes and modifications as defined by the claims and the description herein should be made while remaining within the scope of the invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A preparation method of silica aerogel is characterized by comprising the following steps: comprises the following steps of putting the armorThe structural general formula of the trialkoxysilane is R 1 Si(OR 2 ) Mixing the functional silane coupling agent, absolute ethyl alcohol and deionized water, adding an acid solution for hydrolysis, and then adding an alkali compound for condensation to prepare wet gel; after the wet gel is aged, replacing for 2 times by using a cross-linking agent solution, taking out, cross-linking under ultraviolet irradiation, and drying to obtain flexible silica aerogel; wherein R is 1 Independently selected from vinyl or 3-mercaptopropyl, R 2 Independently selected from methyl, ethyl or isopropyl;
when R is 1 When the cross-linking agent solution is vinyl, the cross-linking agent solution is an absolute ethyl alcohol solution of a mixture formed by mercaptopropyl silicone oil and a photoinitiator, the concentration of the mercaptopropyl silicone oil is 50-200g/L, and the concentration of the photoinitiator is 1-4g/L; the structural general formula of the mercaptopropyl silicone oil is Me 3 SiO(SiMeR 3 O) a (SiMe 2 O) b (SiMeRsO) c SiMe 3 Wherein Me is methyl, R 3 Independently selected from phenyl, methyl, 3-trifluoropropyl, ethyl, n-propyl, isopropyl, isobutyl, n-hexyl, n-octyl, isooctyl, n-dodecyl or n-hexadecyl, rs is 3-mercaptopropyl, a is more than or equal to 0 and less than or equal to 20, b is more than or equal to 10 and less than or equal to 50, and c is more than or equal to 2 and less than or equal to 10;
when R is 1 When the cross-linking agent solution is 3-mercaptopropyl, the cross-linking agent solution is an absolute ethyl alcohol solution of a mixture formed by vinyl silicone oil and a photoinitiator, the concentration of the vinyl silicone oil is 50-200g/L, and the concentration of the photoinitiator is 1-4g/L; the structural general formula of the vinyl silicone oil is Me 3 SiO(SiMeR 4 O) x (SiMe 2 O) y (SiMeViO) z SiMe 3 Wherein Me is methyl, R 4 Independently selected from phenyl, methyl, 3-trifluoropropyl, ethyl, n-propyl, isopropyl, isobutyl, n-hexyl, n-octyl, isooctyl, n-dodecyl or n-hexadecyl, vi is vinyl, x is more than or equal to 0 and less than or equal to 20, y is more than or equal to 10 and less than or equal to 50, and z is more than or equal to 2 and less than or equal to 10.
2. The method of manufacturing according to claim 1, characterized in that: the methyltrialkoxysilane is at least one selected from methyltrimethoxysilane, methyltriethoxysilane and methyltrisopropoxysilane.
3. The method of manufacturing according to claim 1, characterized in that: the molar ratio of the methyltrialkoxysilane to the functional silane coupling agent is 1:0.01-0.2.
4. The method of manufacturing according to claim 1, characterized in that: the volume ratio of the methyltrialkoxysilane to the absolute ethyl alcohol to the deionized water is 1:3-5:0.3-0.6.
5. The method of manufacturing according to claim 1, characterized in that: the photoinitiator is at least one selected from benzoin, benzoin dimethyl ether, benzoin diethyl ether and benzoin butyl ether.
6. The method of manufacturing according to claim 1, characterized in that: the drying is normal pressure drying, and the drying process is that the drying is carried out for 3-5 hours at 40-60 ℃, 3-5 hours at 80-100 ℃ and 2-3 hours at 120-150 ℃.
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| CN111430647A (en) * | 2020-05-08 | 2020-07-17 | 曹亚琼 | High-performance lithium ion battery diaphragm and preparation method thereof |
| CN111592004B (en) * | 2020-05-25 | 2022-04-08 | 福建拓烯新材料科技有限公司 | Preparation method of silicon dioxide aerogel and silicon dioxide aerogel |
| CN112158852B (en) * | 2020-09-29 | 2022-01-28 | 航天特种材料及工艺技术研究所 | High-strength ultralow-density transparent silicon dioxide aerogel and preparation method and application thereof |
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